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1.
Orthorhombic Sc2Mo3O12 films have been successfully prepared via spin coating technique followed by annealing at 500–750 °C. The phase composition, microstructure, morphology and negative thermal behavior of the synthesized Sc2Mo3O12 films were investigated. XRD and XPS analysis indicate that as-deposited film is amorphous. Orthorhombic Sc2Mo3O12 films can be prepared after post-annealing at 500–750 °C for 1 h. The crystallinity of Sc2Mo3O12 films gradually improved with the increase of post-annealing temperature. SEM analysis shows as-deposited film is smooth and compact, and the grain size of Sc2Mo3O12 film grows up as the post-annealing temperature increases. Variable temperature XRD analysis demonstrates that the synthesized orthorhombic Sc2Mo3O12 films show stable thermo-chemical and anisotropic NTE property in 25–700 °C. The corresponding coefficients of thermal expansion (CTEs) of the orthorhombic Sc2Mo3O12 film in a, b and c directions are ?6.68 × 10?6 °C?1, 5.08 × 10?6 °C?1 and ?4.76 × 10?6 °C?1, respectively. The whole unit cell of the orthorhombic Sc2Mo3O12 film shrinks and the volumetric CTE of the Sc2Mo3O12 thin film is ?6.36 × 10?6 °C?1, and the linear CTE is about ?2.12 × 10?6 °C?1 (αv = 3αl).  相似文献   

2.
Al2Mo3O12 is a typical negative thermal expansion (NTE) material, whose thermal expansion behavior depends on its crystal phase. The thermal shock caused by temperature-induced phase transition limits its wide application. The two series of Al2. xScxMo3O12 (0 ≤ x ≤ 1) and Al2Mo3-xWxO12 (0 ≤ x ≤ 2.5) solid solutions with controllable phase transition temperature were synthesized via single cation substitution at the A or B position. The problem of thermal shock caused by the change of temperature is effectively solved in the synthesized Al1.6Sc0.4Mo3O12 and Al2Mo0.5W2.5O12, showing stable NTE performance above room temperature, and the coefficients of thermal expansion of which are ?2.19 × 10?6 °C?1 in 100–550 °C and ?4.25 × 10?6 °C?1 in 85–500 °C, respectively. A-site cation substitution is a more effective way to tune the thermal expansion properties of Al2Mo3O12, which is attributed to the fact that the bond strength of A-O is weaker than that of B–O in the compound.  相似文献   

3.
《Ceramics International》2023,49(19):31627-31633
Orthorhombic In0.5Sc1.5Mo3O12 nanofibers were prepared by electrospinning followed by a heat treatment. The effects of post-annealing temperatures on the phase composition, microstructure and morphology were investigated by XRD, SEM, HRTEM and XPS. Negative thermal expansion (NTE) behaviors of the In0.5Sc1.5Mo3O12 nanofibers were analyzed by high-temperature XRD. Results indicate that the as-prepared In0.5Sc1.5Mo3O12 nanofibers show an amorphous structure with smooth and homogeneous shape. The average diameter of the as-prepared In0.5Sc1.5Mo3O12 nanofibers is around 515 nm. Well crystallized orthorhombic In0.5Sc1.5Mo3O12 nanofibers could be prepared after post-annealing at 550 °C for 2 h with an average diameter of about 192 nm. The crystallinity of In0.5Sc1.5Mo3O12 nanofibers gradually improved with the increase of annealing temperature. However, too high post-annealing temperature leads to a damage of sample's fiber structure. The high-temperature XRD results reveal that In0.5Sc1.5Mo3O12 nanofibers show an anisotropic NTE, and the coefficients of thermal expansion (CTEs) along a-axis and c-axis were −5.95 × 10−6 °C−1 and -3.54 × 10−6 °C−1, while the one along b-axis is 5.61 × 10−6 °C−1. The volumetric CTE of In0.5Sc1.5Mo3O12 nanofibers is −3.90 × 10−6 °C−1 and the linear one is 1.3 × 10−6 °C−1 in 25–700 °C.  相似文献   

4.
《Ceramics International》2022,48(12):16554-16561
Herein, we report the solid-state synthesis of (KMg)xFe2-xMo3O12 (0 = x ≤ 1.5) ceramics. Phase composition, crystal structure, morphology, phase transition and thermal expansion behavior of the (KMg)xFe2-xMo3O12 ceramics were investigated by XRD, Raman, XPS, HRTEM, EDX, SEM, TMA and high-temperature XRD. Results indicate that (KMg)3+ dual-cations have successfully replaced Fe3+ in Fe2Mo3O12 ceramics and single-phase monoclinic (KMg)xFe2-xMo3O12 ceramics were prepared for 0.25 = x ≤ 1. (KMg)3+ introduction can increase the density of (KMg)xFe2-xMo3O12 ceramics and effectively improve their negative thermal expansion (NTE) performance. In addition, the phase transition temperature (Tc) of Fe2Mo3O12 was reduced from 508.1 °C to room temperature with the increase of (KMg)3+-substitution. Monoclinic KMgFeMo3O12 ceramics was observed to show stronger NTE in a wider temperature range of 30–700 °C for the first time. Its corresponding coefficient of thermal expansion (CTE) is as high as ?17.21 × 10?6 °C?1. The distortion of [FeO6/MgO6] polyhedra in (KMg)xFe2-xMo3O12 caused by (KMg)3+-substitution contributed to the stronger NTE.  相似文献   

5.
Recently, a new i-MAX phase with in-plane chemical order has been discovered. In this study, the i-MAX phase (Mo2/3Sc1/3)2AlC and (Mo2/3Lu1/3)2AlC ceramics were synthesized by spark plasma sintering (SPS) with purity up to 96.45 wt% and 95.46 wt%, respectively. Relative densities were up to 98.29 % (M = Sc) and 98.23 % (M = Lu). Microstructure, physical and mechanical properties of (Mo2/3M1/3)2AlC (M = Sc and Lu) ceramics were systematically investigated. Grain sizes of (Mo2/3M1/3)2AlC (M = Sc and Lu) were also counted. The measured coefficients of thermal expansion (CTE) were 8.95 × 10−6 K−1 (M = Sc) and 8.97 × 10−6 K−1 (M = Lu), from 25 °C to 1200 °C. Regarding mechanical properties, the Vickers hardness of (Mo2/3Lu1/3)2AlC was much higher than that of (Mo2/3Sc1/3)2AlC, while the differences in flexural strength, fracture toughness and compressive strength were small. It indicates that both ceramics have good application prospects.  相似文献   

6.
《Ceramics International》2020,46(6):7259-7267
Co-precipitation was successfully applied to synthesize the Sc3+ doped In2-xScx (WO4)3 (x = 0, 0.3, 0.6, 0.9 and 1.2) compounds. The composition- and temperature-induced structural phase transition and thermal expansion behaviors of Sc3+ doped In2(WO4)3 were investigated. Results indicate that In2-xScx (WO4)3 crystalizes in a monoclinic structure at 300 °C for x ≤ 0.3 and changes into hexagonal structure for x ≥ 0.6. Hexagonal In1.1Sc0.9(WO4)3 displays negative thermal expansion (NTE) with an average linear coefficient of thermal expansion (CTE) of −1.85 × 10−6 °C −1. After sintering at 700 °C and above, a phase transition from hexagonal to orthorhombic phase was observed in In2-xScx (WO4)3 (x ≥ 0.6). Sc3+ doping successfully reduce the temperature-induced phase transition temperature of In2-xScx (WO4)3 ceramics from 250 °C (x = 0) to room temperature (x = 0.9). When x = 0.9 and 1.2, the average linear CTEs of In2-xScx (WO4)3 ceramics are −5.45 × 10−6 °C−1 and -4.43 × 10−6 °C−1 in a wider temperature range of 25–700 °C, respectively.  相似文献   

7.
《Ceramics International》2023,49(7):10714-10721
Orthorhombic Sc2(MoO4)3 nanofibers have been prepared by ethylene glycol assisted electrospinning method. The effects of annealing temperature, precursor concentration, spinning distance and solvent on the preparation of Sc2(MoO4)3 nanofibers were characterized by XRD, SEM, HRTEM, EDX and high-temperature XRD. XRD analysis shows as-prepared nanofibers are amorphous. Orthorhombic Sc2(MoO4)3 nanofibers can be fabricated after annealing at different temperatures in 500–800 °C for 2 h. The crystallinity of Sc2(MoO4)3 nanofibers improves and the nanofiber diameter decreases gradually as the annealing temperature increases. However, the nanofiber structure was destroyed at the annealing temperature above 700 °C. Higher precursor concentration results in a slight increase of diameter and decrease in destroying temperature of Sc2(MoO4)3 nanofibers. Spinning distance also affects the diameter of nanofibers, and the nanofiber diameter decreases as the distance increases. One-dimensional orthorhombic Sc2(MoO4)3 nanofibers exhibit anisotropic negative thermal expansion. In 25–700 °C, the coefficients of thermal expansion (CTE) of αa, αb and αc are ?5.81 × 10?6 °C?1, 4.80 × 10?6 °C?1 and -4.33 × 10?6 °C?1, and the αl of Sc2(MoO4)3 nanofibers is ?1.83 × 10?6 °C?1.  相似文献   

8.
《Ceramics International》2023,49(5):7842-7852
Thermal barrier coatings with excellent thermal performance and corrosion resistance are essential for improving the performance of aero-engines. In this paper, (Y3-xYbx)(Al5-xScx)O12 (x = 0, 0.1, 0.2, 0.3) thermal barrier coating materials were synthesized by a combination of sol-gel method and ball milling refinement method. The thermal properties of the (Y3-xYbx)(Al5-xScx)O12 ceramics were significantly improved by increasing Yb and Sc doping content. Among designed ceramics, (Y2.8Yb0.2)(Al4.8Sc0.2)O12 (YS-YAG) showed the lowest thermal conductivity (1.58 Wm?1K?1, at 800 °C) and the highest thermal expansion coefficient (10.7 × 10?6 K?1, at 1000 °C). In addition, calcium-magnesium- aluminum -silicate (CMAS) corrosion resistance of YS-YAG was further investigated. It was observed that YS-YAG ceramic effectively prevented CMAS corrosion due to its chemical inertness to CMAS as well as its unique and complex structure. Due to the excellent thermal properties and CMAS corrosion resistance, YS-YAG is considered to be prospective material for thermal barrier coatings.  相似文献   

9.
Monodispersed flower-like titanate superstructure was successfully prepared by simple hydrothermal process without any surfactant or template. N2-sorption analysis, scanning electron microscopy (SEM), and X-ray diffraction (XRD) observation of as-synthesized product revealed the formation of flower-like titanate with diameter of about 250–450 nm and BET surface area (SBET) of 350.7 m2 g?1. Upon thermal treatment at 500 °C, the titanate nanosheets were converted into anatase TiO2 with moderate deformation of their structures. The as-prepared flower-like titanate showed high photocatalytic activity for H2 evolution from water splitting reaction. Moreover, the sample heat treated at 500 °C exhibited higher photocatalytic activity than that of commercial TiO2 anatase powder (ST-01).  相似文献   

10.
《Ceramics International》2021,47(24):34687-34694
To improve the negative thermal expansion (NTE) performance of ln2W3O12, a novel series of NTE (KMg)xln2-xW3O12 ceramics were fabricated via the solid-state method. The effects of (KMg)3+ substitution on the phase composition, microstructure and thermal expansion property of the ln2W3O12 ceramics were characterized using X-ray diffraction (XRD), Raman spectrometer (Raman), X-ray photoelectron spectrometer (XPS), scanning electron microscopy (SEM), transmission electron microscope (TEM) and thermal mechanical analyzer (TMA). Results indicate that (KMg)3+ can partially replace In3+ in In2W3O12 and form a new phase KxMgxln2-xW3O12 with monoclinic symmetry. For x = 0.5, pure monoclinic (KMg)0.5ln1.5W3O12 ceramics is prepared and shows strong NTE. Its coefficient of thermal expansion is −7.89 × 10−6 °C−1 in 30–700 °C, in addition, no phase transition was observed over the entire testing temperature range. These research results indicate that double cations co-substitution is an effective strategy to improve the NTE property of ln2W3O12 through crystal structure modulation. This strategy could be extended to the performance modulation of other NTE materials.  相似文献   

11.
In(HfMg)0.5Mo3O12, which can be considered as a 1:1 mole ratio solid solution of the low‐positive thermal expansion material HfMgMo3O12 and the low‐negative thermal expansion (NTE) material In2Mo3O12 was prepared. From DSC and XRPD results, we show that In(HfMg)0.5Mo3O12 exists in a monoclinic (P21/a) structure at low temperature and undergoes a phase transition at ~425 K to an orthorhombic phase (Pnma), with an associated enthalpy change of 0.89 kJ mol?1. Thermal expansion is large and positive in the low‐temperature monoclinic phase (average α? = 16 × 10?6 K?1 and 20 × 10?6 K?1, from dilatometry and XRPD, respectively). Remarkably, this material has a near‐zero thermal expansion (ZTE) coefficient over the temperature range ~500 to ~900 K in the high‐temperature orthorhombic phase, both intrinsically and for the bulk sample. The average linear intrinsic (XRPD) value is α? = ?0.4 × 10?6 K?1, and the average bulk (dilatometric) value is α? = 0.4 × 10?6 K?1 with an uncertainty of ± 0.2 × 10?6 K?1. The slight difference between intrinsic and bulk thermal expansion is attributed to microstructural effects. XRPD results show that the thermal expansion is more isotropic than for the parent compounds HfMgMo3O12 and In2Mo3O12.  相似文献   

12.
The different alumina whiskers phases are extensively used to reinforce high-performance composite materials. The understanding of the mutual relationship of the different phases is key for simulating Al2O3 whiskers containing systems and is of general interest for the metal oxide and ceramic communities. In this paper, we used homogeneous precipitation to synthesized flower-like boehmite whisker precursors from aluminum sulfate and urea. The synthesized precursors were calcined at 600, 900, and 1200 °C to obtain flower-like whiskers of γ-, θ-, and α-Al2O3 phases, respectively. The precursor boehmite crystals prepared in closed, semi-closed, and open reactor systems were qualitatively analyzed using SEM. The results showed that the usea hydrolysis, which serves as a source of OH? ions, is slow under closed-reactor conditions, which favors the growth of the boehmite crystal nuclei into whiskers. We adopted the L16 (43) orthogonal design of experiment to analyze the influence of reaction temperature, time, and the amount of urea (relative to the amount of Al2(SO4)3) in the closed system. Synthesis temperature of 160 °C and the processing time of 8 h yielded optimal boehmite flower-like whiskers. Physicochemical properties of the precursor and series of alumina phases were characterized using thermogravimetric/differential thermal analysis (TG/DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM) methods. Finally, the obtained results and the thorough analysis of the growth mechanism suggested the step-growth model of boehmite flower-like whiskers.  相似文献   

13.
The effects of the presence of Ga2O3 on low‐temperature sintering and the phase stability of 4, 5, and 6 mol% Sc2O3‐doped tetragonal zirconia ceramics (4ScSZ, 5ScSZ, and 6ScSZ, respectively) were investigated. A series of zirconia sintered bodies with compositions (ZrO2)0.99?x(Sc2O3)x(Ga2O3)0.01, x = 0.04, 0.05, and 0.06 was fabricated by sintering at 1000°C to 1500°C for 1 h using fine powders that were prepared via the combination of homogeneous precipitation method and hydrolysis technique using monoclinic zirconia sols synthesized through the forced hydrolysis of an aqueous solution of zirconium oxychloride at 100°C for 168 h. The presence of 1 mol% Ga2O3 was effective in reducing sintering temperature necessary to fabricate dense bodies and enabled to obtain dense sintered bodies via sintering at 1100°C for 1 h. The phase stability, that is, low‐temperature degradation behavior of the resultant zirconia ceramics was determined under hydrothermal condition. The zirconia ceramics codoped with 1 mol% Ga2O3 and 6 mol% Sc2O3 (1Ga6ScZ) fabricated via sintering at 1300°C for 1 h showed high phase stability without the appearance of monoclinic zirconia phase, that is the tetragonal‐to‐monoclinic phase transformation was not observed in the 1Ga6ScZ after treatment under hydrothermal condition at 150°C for 30 h.  相似文献   

14.
Bi(Sc1/3Mo2/3)O4 ceramics were prepared via solid state reaction method. It crystallized with an ordered scheelite-related structure (a?=?16.9821(9)?Å, b?=?11.6097(3)?Å, c?=?5.3099(3)?Å and β?=?104.649(2)°) with a space group C12/C1, in which Bi3+, Sc3+ and Mo6+ are ?8, ?6 and ?4 coordinated, respectively. Bi(Sc1/3Mo2/3)O4 ceramics were densifiedat 915?°C, giving a permittivity (εr) ~24.4, quality factor (Qf, Q?=?1/dielectric loss, f?=?resonant frequency) ~48, 100?GHz and temperature coefficient of resonant frequency (TCF)?~??68?ppm/°C. Impedance spectroscopy revealed that there was only a bulk response for conductivity with activation energy (Ea) ~0.97?eV, suggesting the compound is electrically and chemically homogeneous. Wide band dielectric spectra were employed to study the dielectric response of Bi(Sc1/3Mo2/3)O4 from 20?Hz to 30?THz. εr was stable from 20?Hz to the GHz region, in which only ionic and electron displacive polarization contributed to the?εr.  相似文献   

15.
Negative thermal expansion (NTE) performance of Fe2(MoO4)3 is only found in a high-temperature range due to its monoclinic-to-orthorhombic (M-O) phase transformation temperature (PTT) at 503.5°C. To stabilize the orthorhombic phase of Fe2(MoO4)3 at room temperature, a series of Fe2-xScx(MoO4)3 (0≤x≤1.5) (abbreviated as F2-xSxM) were fabricated via solid-state reaction. Results indicate that the M-O PTT of Fe2(MoO4)3 is successfully reduced from 503.5°C to 34.5°C by A-site cation substitution of Sc3+. The regulation mechanism is considered to be the decrease in electronegativity of (Fe2-xScx)6+ in F2-xSxM. Both variable temperature X-ray diffraction (XRD) and thermal mechanical analysis (TMA) analysis results indicate that F0.5S1.5 M exhibits anisotropic NTE in 100–700°C. The results indicate that it can effectively improve the densification of Sc-substituted F0.5S1.5 M ceramics by two-step calcination process. Furthermore, higher second-step calcination temperature is beneficial for the formation of single-phased orthorhombic F0.5S1.5 M. The NTE response temperature range of F0.5S1.5 M ceramics second-step sintered at 1000°C is broadened to 30–600°C, and the corresponding coefficient of thermal expansion is -5.74 × 10−6°C−1. The ease in the proposed design and preparation method makes NTE F0.5S1.5 M potential for a wide range of applications in precision mechanical, electronic, optical, and communication instruments.  相似文献   

16.
Fe2-xAgxO3 (0?≤?x?≤?0.04) nanopowders with various Ag contents were synthesized at different hydrothermal reaction temperatures (150?°C and 180?°C). Their structural properties were fully investigated through an X-ray diffraction, a Fourier transform infrared spectroscopy, and an X-ray photoelectron spectroscopy. The hydrothermal reaction temperature, time, and Ag content remarkably affected the morphological characteristics and crystal structure of the synthesized powders. The Fe2-xAgxO3 (0?≤?x?≤?0.04) powders synthesized at 150?°C for 6?h and the Fe2-xAgxO3 (0.02?≤?x?≤?0.04) powders synthesized at 180?°C for 12?h formed the orthorhombic α-FeOOH phase with a rod-like morphology, whereas the Fe2-xAgxO3 (0?≤?x?≤?0.01) powders synthesized at 180?°C for 12?h formed the rhombohedral α-Fe2O3 phase with a spherical-like morphology. The Fe1.98Ag0.02O3 fabricated by utilizing Fe1.98Ag0.02O3 powders synthesized at 180?°C showed the largest power factor (0.64?×10?5 Wm?1 K?2) and dimensionless figure-of-merit (0.0036) at 800?°C.  相似文献   

17.
A new series of rare earth solid solutions Sc2−xYxW3O12 was successfully synthesized by the conventional solid-state method. Effects of doping ion yttrium on the crystal structure, morphology and thermal expansion property of as-prepared Sc2−xYxW3O12 ceramics were investigated by X-ray diffraction (XRD), thermogravimetric analysis (TG), field emission scanning electron microscope (FE-SEM) and thermal mechanical analyzer (TMA). Results indicate that the obtained Sc2−xYxW3O12 samples with Y doping of 0≤x≤0.5 are in the form of orthorhombic Sc2W3O12-structure and show negative thermal expansion (NTE) from room temperature to 600 °C; while as-synthesized materials with Y doping of 1.5≤x≤2 take hygroscopic Y2W3O12·nH2O-structure at room temperature and exhibit NTE only after losing water molecules. It is suggested that the obvious difference in crystal structure leads to different thermal expansion behaviors in Sc2−xYxW3O12. Thus it is proposed that thermal expansion properties of Sc2−xYxW3O12 can be adjusted by the employment of Y dopant; the obtained Sc1.5Y0.5W3O12 ceramic shows almost zero thermal expansion and its average linear thermal expansion coefficient is −0.00683×10−6 °C−1 in the 25–250 °C range.  相似文献   

18.
《Ceramics International》2015,41(8):9873-9877
Solid solutions of In2−xScxW3O12 (0≤x≤2) were successfully synthesized using the solid state reaction method. Effects of substituted scandium content on the phase composition, microstructure, phase transition temperatures and thermal expansion behaviors of the resulting In2−xScxW3O12 (0≤x≤2) samples were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and thermal mechanical analyzer (TMA). Results indicate that the obtained In2W3O12 ceramic undergoes a structure phase transition from monoclinic to orthorhombic at 248 °C. This phase transition temperature of In2W3O12 can be easily shifted to a lower temperature by partly substituting the In3+ with Sc3+. When the x value increased from 0 to 1, the phase transition temperatures of In2−xScxW3O12 (0≤x≤2) samples decreased from 248 to 47 °C. All the In2−xScxW3O12 (0≤x≤2) ceramics show fine negative thermal expansion below their corresponding phase transition temperatures. The negative thermal expansion coefficients of the In2−xScxW3O12 (0≤x≤2) ceramics change in the range from −1.08×10−6 °C−1 to −7.13×10−6 °C−1.  相似文献   

19.
A 2024Al metal matrix composite with 10?vol% negative expansion ceramic ZrMgMo3O12 was fabricated by vacuum hot pressing, and the influence of sintering temperature on the microstructure and thermal expansion coefficient (CTE) of alloys was investigated. Experimental results showed that all ZrMgMo3O12p/2024Al composites sintered at 500–530?°C had a similar reticular structure and exhibited different linear expansion coefficients at 40–150?°C and 150–300?°C. The addition of 10?vol% ZrMgMo3O12 decreased the CTEs of 2024Al by ~ 16% at 40–150?°C and by ~ 7% at 150–300?°C. This addition also increased the hardness of 2024Al by ~ 23%. The density of the composites and the content of Al2Cu in ZrMgMo3O12p/2024Al increased as the sintering temperature increased. The CTEs of the composites decreased, whereas hardness increased. Thermal cycling from 40?°C to 300?°C caused the CTEs of the composites to decrease gradually and reach a stable value after seven cycles. The lowest CTEs of 15.4?×?10?6 °C?1 at 40–150?°C and 20.1?×?10?6 °C?1 at 150–300?°C were obtained after 10 thermal cycles and were reduced by ~ 32% and ~ 17%, respectively, compared with the CTE of the 2024Al. Among the current reinforcements, ZrMgMo3O12 negative expansion ceramics showed the highest efficiency to decrease the CTE of Al matrix composites.  相似文献   

20.
A method for synthesizing YSAG:Yb optical ceramics has been developed. Additionally, the phase composition and unit cell parameters for YSAG, YbSAG, and their solid solutions have been determined. The limits of scandium solubility in the dodecahedral and octahedral sites of garnet crystal lattice have been estimated after annealing at 1600°C. The scandium solubility limit in the dodecahedral sites of YSAG:Yb was found to be 66 ± 2 at.%. The limit of scandium solubility in octahedral sites depended upon the type of garnet-forming cations. The solubility limit for Sc3+ decreased from 97.5 ± 0.5 to 68.5 ± 1 at.% with simultaneous increase of ytterbium content in the YSAG-YbSAG system. Therefore, the region of solid solutions existing with a garnet structure in the Al2O3–Sc2O3–Yb2O3–Y2O3 system was determined. Samples having scandium in both dodecahedral and octahedral sites, which had a Sc3+ content of ~30 at.%, were synthesized as a precursor for optical ceramic production.  相似文献   

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